Chlorotrimethylsilane → HCID 68509351, 화합물
반응식
[CH2:1]([C:3]1[NH:7][N:6]=[C:5]([C:8]([OH:10])=[O:9])[C:4]=1[CH3:11])[CH3:2].[Cl:12][Si](C)(C)[CH3:14]>CO>[ClH:12].[CH2:1]([C:3]1[NH:7][N:6]=[C:5]([C:8]([O:10][CH3:14])=[O:9])[C:4]=1[CH3:11])[CH3:2]참가 물질
4
실험 절차
To a mechanically stirred suspension of 5-ethyl-4-methyl-1H-pyrazole-3-carboxylic acid (1.0 g, 6.49 mmol) in dry methanol (30 mL) was added chlorotrimethylsilane (2.5 mL, 19.5 mmol). The reaction mixture was heated at reflux over night. After being cooled to rt, the solvent was removed in vacuo, and the residue was stirred in diethyl ether (20 mL) for 1 h. After filtration and vacuum drying the title compound was obtained as white crystals (832 mg, 63%): 1H NMR (400 MHz, CDCl3) δ 10.55 (broad, 1H), 4.00 (s, 3H), 2.91 (quart, 2H), 2.32 (s, 3H), 1.35 (t, 3H); ES-MS m/z 169 (MH)+; HPLC RT (Method F) 1.52 min.
후처리
- temperatureThe reaction mixture was heated
- temperatureat reflux over night
- customthe solvent was removed in vacuo
- filtrationAfter filtration and vacuum
- dry with materialdrying the title compound
출처 및 근거
- ORD 기록
- ord-dc22f6aec5d44ffebf4cb8fd80b5ef2d
- 출처 데이터셋
- uspto-grants-2014_08
- 특허 번호
- US08796253B2
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